Process and apparatus for purifying camphob



March 4 1924.

E G. LOOMIS PROCESS AND APPARATUS FOR PURIFYING CAMFHOH 2 Shams-Sheet 1Filed March 16, 1918 I? Y Phi/Mia Mm" E. G. LOOMIS PROCESS AND APPARATUSFOR PURIFYING CAMPHOR March 4 1924.

Filed March 16, 1918 2 Sheets-Sheet 2 IN VEN TOR. fl -m W I A TTORNE)Patented Mar. 4, 19%4.

UNITED STATES PATENT OFFICE.

EVAR'IS G. LOOMIS, OF NEWARK, NEW JERSEY, ASSIGNOR T E. I. DU FONT DENEMOURS AND COMPANY, OF WILMINGTON, DELAWARE, A CORPORATION OF DELAWARE.

PROCESS AND APPARATUS FOR PURIFYING CAMPHOB Application filed March 16,1918. Serial No: 222.859.

T0 altar/1 0m it may concern.

Be it known that I, Evnn'rs i. LooMrs. of Newark, in the county of Essexand in the State of New Jersey, have invented a .59 certain new anduseful Improvement in Processes and Apparatus for Purifying Camphor, anddo hereby declare that the following is e full. clear, and exactdescription thereof;

The ohject of my invent n has been to provide a proiess and apparatusfor practicing such process, lrv which comphor may he purified rapidlyand at low cost. and especially sur-h ii process and apparatus by whichcrude cmnphor can he introduced continuously into the nppnrutus andrelined cun'iphor (:ontinurnisly removed therefrom. whereby a largeoutput and low cost for labor and heat is obtained.

In .the accompanying drawing is shown. sqnieu hut diagrammatically, an.apparatus emhod ing my invention, which, while it is the hostembodiment known to me. is to be regarded as typical only of manypossihle embodiments, and my invention is not to heconfined thereto.

In the said drawings.

Fifiure 1. is a vertical longitudinal sec tionnl' view of an apparatusemhodying my invention;

Figure 2 is i1 top plan view of the apparatus shown in Figure l;

Figure 3 is a vertical sectional View of the camphor condenser on theline 3-3 of Figure l.

Qamphor contains as impurities cumphor oil. resinous impurities. waterand dirt. Prior to my invention. camphor. to hepurified. has beensubjected to a heating .op-

i eration, which has the effect of changing the character of the camphoroil so as to p'rmi-t'itto be readily separated from the camphor. By myinvention. however, such process can be greatly facilitated.

The apparatus shown in the accompanyinn drawing"comprises a meltingpot 1. in which the crude camphor. is to be melted. Means forintroducing the camphor into the pot without permitting the vapors ofticumphor to escape, as shown. consist of a hopper '2. into which thecrude cainphor is conveyed in any manner, and the eamphor is fedhorizontally. as by a screw conveyor 4, to a vertical pipe 0,communicating with the interior of the melting' pot, the pipe 5 having;-within it a screw conveyor 6, which takes the camphor from the conveyer4 and forces it into the melting pot. The melt in: pot is heated in anydesired manner and is shown as heated by interior piping 7 convcfyinghot oil. The piping system will later he described. .-\t a point at alevel preferably above the melting pot. a steam condenser 8 is provided,and 11 pipe 9 extends from the upper end of the melting pot into, therondenser to carry (iii any vapors of water. eamphor or czimphor oilthat may he formed in the melting pot. In the present instance, thecondenser is shown as provided with a Water spray S at the top. suppliedby a pump 8*. The condenser is provided at its foot with a water seal8". The screws 4 and G and pump 8" are shown as driven by a horizontalshaft 8". The lower end of the melting pot is connected by it pipe ll)with the lower end of a vaporizer l1. 1 prel'cr that the pipe 10 shouldslope downward considered in a. direction toward the vaporizer. andbelieve-that I obtain ii more suncessl'ul linking: and transformation ofthe impurities and a, more ready separation of them from the camphorthan if the pipe he level or slope upward. The pipe 10, as

well as the melting pot, heated with a hot oil heating system,pretcruhly internal. The hot oil heating system. as illustrated.consists of a pipe 12 passing: through the pipe 10, andopening againstthe closed end of a larger pipe 13. which encloses the pipe 12. andwhich. itself. is contained within the pipe 10. The pipe 13 serves toreturn the oil to 21 head 14. where it. passes into a pipe 15 that ri esinto the melting pot and forms the coil 7, the upper end of which coil,in a pipe 17, connects with a pipe 18 that is contained within the pipeEL connecting the melting pot with the water condenser. and the oil.after rising to the top of the pipe 18. desrends through an internalpipe1!) and returns to the heater.

The czunphor is largely baked in its passage through the pipe 1". whichis of such :1 length that the desired amount of time is consumed in thepas age of the rnmphor lheretlu-ourrh to effect the baking, Within thethe loner end of the vaporizer a sufficient Bod of the molten camphor isretained to m a liquid seal over the end The va orizer is of the pipe10, and prevent the vapors of camphor from passing back into the.melting pot and'attempting to escape through the entrance thereto, butin the upper part of the vaporizer vapors of camphor are formed and,after passing through the scrubber 20, are carried oil through a pipe 21to a condenser 22 of any desired form. heated by a hot on] pipe 23 preerably contained within the, vaporizer, and constructed in the form ofacoil 24. -The upper end of the coil is connected is there melted, and, at

by a pipe that heats the connection 28 to the scrubber. 1

In the operation ofthe described apparatoe in the refining of camphor,the crude camphor in the hopper 2 is fed horizontally forward by thescrew conveyor 4 to the vertical screw conveyor 6, which latter feeds itdown into the melting pot. The camphor hongh fumes of camphor rise tosomfljcxtent and tend to escape past the scmwtconveyers, the mass of camhor, carried by the conveyers condenses t e fumes so that practical! nocam-.

' phor is lost in this way. The me ting vesthe pipe 10 to the vs thancamphor 1 flows through the pipe 10 the vaporizer 11 and carries with itthe sol is kept at a temperature above the melting point of camphor andbelow its boiling int, so asboth to melt the'cnmphor and The vaporswhich escape to the condenser 8, therefore, contain only a smallpercentage of camphor, together with a httle of the camphor oil. Thevapors passing into the condenser 8 are condensed by the spray of waterand the the said pipe phor oil and resinous matters are modjfiedieitherinto non-volatile s'u slices or substances which have a diflerentvolatility or both) and b chan in the su tances, ey can se amte from thecamphor. The camp or into .the'foot'of altered impurities, which lattersettle'in the footfof the vaporizenifrom which theyare moved from timeto time. The liquid camphor in thelower portion of the vaporizer isheated to such a point that'vapors of cumphor rise from its surface,and, vassing through the scrubber and through t e pipe these eel 21,pass 01! into the condenser 22, and may be then carried out of thecondenser by a screw oonveyer 27. As convent-ionall dicated in Figure 1,the scrubber is o; the standard annular-pan bubblel type so that; assome of the camphor vapors are condensed in the upwardly facing pans,the remainder of the vapors, deflect-ed into-the upwardly facing pans bythe downwardly facing pans, use under the of the latter and bubble throuthe liquid calm phor in the upwardly acing pans andBo are scrubbed.

The scrubber is she oil jacket 20 supplied The pipe 21 is heated byreturn-flow oil pipes similar to the pipes 12 and 13 and the pipe 10,the oil being sup pipe 20", leading from theoil acket, and escaping-by api V 21'.

Myinvention lifts, among others, the fol lowing advantages:

The camphor, beingbaked at a temperature above the melting point, ismuch more readily heated to the baking point than if it were baked in asolid condition, since the convection currents communicate the heat tothe mass, camphor in a solid state being a very'pobr conductor of heat.

Baking the car'nphor in the molten condiwn as heated by an i with oil bythe pipe plied by a tion also facilitates transferring the cum I phor tothe next part of the apparatus, and makes possible that continuity ofthe process which is one of the prime objects of my invention. Theseparation of the caluphor from its. impurities bydisti'llin r it, nudesI cially after it has been baked in a 11min:

condition, results in the advantage of the heat already in the oomph-or.I y process is a continuous one, in that camphor can be steadily rinduniformly fedinto the apparatus. beginning with the n elting. pot, andcan be made to pass continuously through the apparatus to the condoneSet, and can 'be conveyed from the latter bythe conveyor-27 continuouslyor at sutli ciently frequent inter rals to prevent the condenser frombecoming filled. This oonti nuity enormously increases the amount of'caniphor which can be refined in a vet:

apparatus compared with intenmitten y res fining it, and it results in alarge savin of best, since the parts which bakeund "fiery wise treat theeaunphor in a heated condition are. not alternately I claim: 1

.1. An apparatus for compri ing a melting vessel, a akmgvescommunicating therewith. means.-- for heating opened and closed l andtherefore are not periodically'chilled or reduced in temperaturepurifying campho'r said two vessels. and a vaporizer communicating withsaid baking vessel, said and again-warmedheating means being locatedwith to said baking vessel for prevention of cooling of the meltedcamphor in its passage from the melting through the baking vessel to thevaporizer, and the baking vessel and the vaporizer being relativelyassembled and located to provide for the maintaining of a body of moltencamphor in said vaporizer in sealing relation to said baking vessel.

:2. An apparatus for purifying camphor comprising the combination of amelting vessel, a water condenser connected therewith, a baking vesselconnected with said melting vessel. and a vaporizer connected with saidbaking: vessel. said baking vesscl and vaporizer beinp relativelylocated to @provide for the maintaining of a bodycf molten camphor insaid vaporizer in sealing relation to said baking vessel.

3. An apparatus for purifying camphor comprising, the combination of amelting vessel, a spray condenser connected therewith, a baking. vesselconnected with said melting vessel. and a vaporizer connected with saidbaking vessel, said baking vessel and vaporizer being relatively locatedto provide for the maintaining of a body of molten camphor in saidvaporizer in sealing relation to said baking vessel.

4. An apparatus for purifying camphor comprising: a meltingvessel formelting the camphor to a liquid. a camphor-rctaining entrance to saidvessel, abovethe normal level of the liquid camphor in said vessel. tohold camphor in amount to close the same, means for Feeding: theretained and closing camphor through said entrance. :1

baking vessel communicating.with said. melting vessel to receive liquidcamphor therefrom. and a vaporizer connected to the 0 baking vessel.

. 5. An apparatus for purifying camphor comprising the. combination of amelting vessel for melting: the camphor-to a liquid. a camphor-retaining entrance to said vessel, above the normal level of theliquid camphor in said vessel. to hold camphor in amount to close thesame. means for feeding theretained and closing. camphor through saidentrance, a. condenser nectedwith said melting vessel. a bakingczvcsselconnected. to said melting vessel for receiving liquidcamphortherefrom. and a vaporizer connected to said baking vessel.

6. An apparatus for purifying camphor comprising the combination of amelting vessel. a camphonretaining entrance thereto. to hold camphor inamount to close the same, means for feeding the retained closingcamiphor through said entrance, a

condenser connected with said melting ves csel; a baking vesselconnected to said melting vessel; n vaporizer connected to said bakingvessel. and a crubber connected with said vaporizer. v

7. An apparatus for purifying cam phor and comprising the combination ofa melting vessel, a camph'or-retaining'entrance thereto, to holdcamphorin amounfito close the same. means for feeding the retained andclosing camphor through said entrance. a

condenser connected with said melting vessel. a baking vessel connectedto said melting vessel; a vaporizer connected to said baking vessel, ascrubber connected with said vaporizer. and a condenser connected withsaid scrubber.

8. An apparatus for purifying camphor comprising the combination ofamelting vessel. a baking vessel connected with said melting vessel. avaporizer connected with said baking vessel. a scrubber connected withsaid vaporizer, and a condenser connected with such scrubber.

9. An apparatus fo purifying camphor comprising the combination of,amelting vessel. a baking vessel connect-ed with said melting vessel. avaporizer connected with said baking: vessel. a j-ubber connected withsaid vaporizer. a fli indenser connected with such scrubber :ifil-'tnezins for convey lug condensed camphor from said condenser.

10. An apparatus for purifying campho'r comprising the combination of amelting vessel, a baking; vessel connected with said melting vessel, :1vaporizer connected with said baking vessel, a scrubber connected withsaid vaporizer, a condenser connected with such scrubber. and mean forpositively movingsolid condensed calnphor from said condenser, saidmeans comprising a screw.

conveyor. 7

11. An apparatu for purifying camphor comprisinp the combination of amelting pot, a vaporizer, and apipe connecting them, and means forheating said pipe to bake camphor while passing therethronph, saidheating means and said pipebeing located with respect to each other forprevention of cooling and solidifying of the cnmphor during its flowfrom the pot to the vaporizer.

12. An apparatus for purifying camphor comprising the combination of amelting; pot. a vaporizer. a pipe connecting them. and means for heatingsaid pipe to bake camphor- 'while passing therethrouglr. said pipesloping toward the vaporizer with its ends at difi'erent levels.

13. An apparatus for puri h comprising-the combination of a me ting pot,a vaporizer. a pipe connecting them. and means for heating said pipe to.bake camphor while passinp therethrouirh. such means comprising meansfor circulating a heating fluid along the length of said pipe. said.pipe sloping towardt-he vaporizer with its ends at different levels.

14 An apparatus for purilfvine (amnhm comprising the combination of amelting pot, a vaporizer. a. pip: connecting them.

1 in" cam hor Hill and means for heating said pipe, to bake camphorwhile passing therethrough, said pipe sloping toward the vaporizer withits ends at diiferent levels.

15. An apparatus for purifying-cam hor' comprising the combination of ame ting pot, a vaporizer. a pipe connecting them, and means for heatingsaid ipe to" bake camphor while passing there; rough, said pipe slopingdownward in a forward direction with its ends at difl'erent levels.

16. The continuous process of refining camphor which comprises theprogressive treatment of successive portions thereof bv' heating thecamphor by applying heat to the camphor at a. temperature above themelting point, and baking it at a temperature below the vaporizingpoint, and performing such heating and baking as so rate and distinctsteps; whereby the ifferent and successive portions of cum hor may besimultaneously treated, each in a respective one of the progressivesteps.

17. The continuous process of refining camphor which comprises theprogressive treatment of successive portions thereof by heating thecamphor by applying heat to the camphor at a temperature above themelting point, baking it at a temperature below'the vaporizing point,and separating the impurities. and performing such heating. baking andseparating as separate and distinct steps; whereby the different andsuccessive portions of camphor may he simultaneously treated, /each ina. resp'ctive one of the progressive steps.

18. The continuous process of refining camphor which comprises theprogressive treatment of successive portions thereof by heating thecamphor by applying heat to V the camphor at a temperature .above themelting .point, baking it at a temperature below the vaporizing point,and vaporizing the camphor, and performing such heating. baking andvaporizing as so arate and distinct steps; whereby the di erent and successive portions of camphor may be simultaneously treated, each in a'respective one of the progressive steps. y

.19. The continuous process of refining camphor which comprises theprogressive treatment of successive portions thereof by heating thecamphor by applying heat to the camphor at a temperature above'themelting "point, baking it at .a'temperature below the vaporizing point,and vaporizing and scrubbing the cam.phor,"and performing such heating,baking, vaporizing and scrub hing asseparate and istinct.-'steps whercbythe difl'erentand camphor may be simultaneously treated, each in arespective one of the progressive ste s.

2%; he continilous process of refining .which comprises the progressiveccssive portions -of treatment of successive portions thereofby heatingthe camphor by applying heat to the camphor at a. tem melting point,baking it at a temperature belou the vaporizing point, vaporizin thecamphor, and condensing the same, an per rature above the the camphor atatemperature above the melting point, baking it at a temperature belowthe vaporizing point. vaporizing and scrubbing the camphor, andcondensin the same, and performing such heating, be ing,. vaporizing andscrubbing, and condensing as separate and distinct .ste whereby thedifl'erent and successive ortions of camphor may be simultaneouslytreated, each in a respective one of the progressive steps.

22. The continuous process of refining camphorcomprising continuouslyand progressive'ly melting the' camphr, and continuously and progressivey ha-king the camp'hor at a di'flerent location from that in which itwas melted. j

23. The conti ous process of purifying camphor I I gressively in ting;the camphor', baking the camphor i n di in which-"it was melted, andprogressively and continuously separating the camphor from itsimpurities. V

24;. The continuous process of purifying camphorcomprising continuouslyand progressively me tiniz the cam-phor; baking the campho'r in a"'difl'erent location from that .in which it was melted, progressively andcontinuously separating, the camphor from its impurities. andprogressively and continuouslysolidifying the camphor. I

25. The. continuous Process of purifying camphor comprising meltingcrude camhor, and separating the volatile impurities,-

aking-a continuous current of'thc .molteh' torrent location'from thatcamphor", and vaporizing saidvcurrent oi baked molten camphor whilepreventing the vapors of camphor from passing into the melting vessel.

26, The continuous process of purifying camphorieomprising melting crudecamnhor,

and separating and condensing the volatile impurities, baking acontinuous current of the molten camphoriand vaporizing said:

current of baked molten camplh'orwhile pre [venting the vapors of camporlfrom passingyback' into the melting vessel; V

ZTrThB continuous process of purifying camphor comprising continuouslymelting a. 9

continuous stream of crude camphor, and separating and condensing thevolatile impurities, baking a continuous current of the vaporizing saidcurrent of baked molten camphor While preventing the vapors of caniphorfrom passing back into the melting vessel.

28. The continuous process of purifying camphor comprising melting crudecamphor, and separating the volatile impurities, baking a continuouscurrent of the molten camphor, vaporizing said current of baked moltencamphor While preventing the vaporsof camphor from passing back into themelting vessel, anthscrubbing said vapors of camphor.

29. The continuous process of purifying camphor comprising melting crudecamphor, and separating and condensing the volatile impurities, baking acontinuous current of the molten cam phor, vaporizing said current ofbaked molten camphor while preventing the vapors of camphor from passingback into the melting vessel, and scrubbing said vapors of camphor,

30. The continuous process of purifying camphor comprising continuouslymelting a continuous stream of crude camphor, and separating andcondensing the volatile impurities, baking a continuous current of themolten campbor, vaporizing said current of baked molten camphor whilepreventing the vapors of camphor from passing back into the meltingvessel, and scrubbing said vapors of camphor.

31. The continuous process of purifying camphor comprising melting crudecamphor, separating the volatile impurities, baking a continuous currentof the molten camphor, vaporizing said current of baked molten camphorwhile preventing the. vapors of camphor from passing back into themelting vessel, scrubbing said vapors of cam phor, and condensing saidscrubbed vapors of camphor.

32. The continuous process of purifying camphor comprising meltingcrudecamphor, separating and condensing the volatile impurities, baking acontinuous current of the molten czunphor, vaporizing said current ofbaked molten camphor while preventing the vapors of camphor from passingback into the melting vessel, scrubbing said vapors of camphor, andcondensing said scrubbed vapors of cainphor.

33. The continuous process of purifying cainphor comprising continuouslymelting a continuous stream of crude camphor, separating and condensingthe volatile impurities, baking u. continuous current of the moltencumphor, vaporizin said current of baked molten camphor \vhi epreventing the vapors of camphor from. passing back into the meltingvessel, scrubbing said vapors of camphor, and condensing said SCI! bedvapors ot' camphor. I

In testimony that I claim the foregoing I have hereunto set my hand.

EVARTS Ur. LOOMIS.

Witnesses:

RUTH J. RIEMAN, J. Fnaonmvvom...

